盐酸雷尼替丁的共振光散射新体系研究及其分析应用

在酸性条件下,盐酸雷尼替丁、铬黑T和钼酸铵通过静电作用形成三元离子缔合物,使体系的共振光散射明显增强.据此建立了共振光散射测定盐酸雷尼替丁的新方法.在最佳条件下,体系的最大散射峰位于363 nm处.共振光散射增强的程度与盐酸雷尼替丁的浓度呈良好的线性关系.方法的线性范围在0.015～0.165 mg/mL,检出限为9.5×10-3 mg/mL.将该方法用于市售盐酸雷尼替丁片的测定,并与药典方法进行对照,证明两种方法之间无显著性差异.     

Study on the interaction of DNA with resveratrol by resonance light scattering technique and its analytical application

The interaction between resveratrol and DNA has been studied by resonance light scattering (RLS) technique. In strongly acidic solution, resveratrol has a maximum peak at 368 nm and the RLS intensity is remarkably enhanced by trace amounts of DNA due to its interaction with resveratrol. Based on this, a novel assay for nucleic acids has been developed. The characteristics of RLS, fluorescence and UV-VIS absorption spectra, the influential factors and optimum conditions of the reaction have been studied. The enhanced RLS intensity at 368 nm is proportional to the concentration of DNA within the range of 0–1600 μg/L for calf thymus DNA. The determination limit (3σ) is 5.2 ng/mL. The study of foreign substance effect on the determination of DNA indicates that most of metal ions have little effect on the determination of DNA. Three synthetic samples of DNA were analysed with satisfactory results. The results show that the proposed method is very sensitive, convenient, rapid and reproducible.     

共振光散射光谱研究噻嗪红R与牛血清白蛋白的作用及其分析应用

研究了噻嗪红R(Thiazine red R,TR)与牛血清蛋白(BSA)作用的共振光散射(RLS)光谱特征。考察了各种影响因素,并计算出了BSA与TR的结合比(质量之比)为1.25。结果表明,在优化条件下体系的RLS强度与蛋白质浓度在一定范围内具有良好的线性关系,据此建立了一种蛋白质测定的新方法。在最佳实验条件(TR,2.0×10-5mol/L;pH2.36)下,BSA的线性范围是0.01~5.0μg/mL,检出限为1.4ng/mL。该方法已用于合成样品及尿液的测定。     

偶氮胭脂红G共振光散射法测定羟自由基的研究及应用

基于Fenton反应产生的·OH对偶氮胭脂红G(AG)的褪色反应,使偶氮胭脂红G在434 nm处共振散射光强度降低,采用偶氮胭脂红G为指示剂,在优化测定条件后,建立了一个共振光散射法测定Fenton反应所产生的·OH的新方法,并用所建立的新方法研究了一些常见抗氧化剂对·OH清除的量效关系,验证了方法的可行性.在此基础上,用该方法研究了一些茶叶水提取液的抗氧化能力,结果表明,所有茶叶提取液均具有一定清除·OH的能力.在所研究的几种茶叶中,以普洱茶清除·OH的能力最强.     

Determination of deoxyribonucleic acids by a resonance light scattering technique and its application

For the first time, acetamiprid has been used to determine nucleic acid (DNA) using the resonance light scattering (RLS). The RLS of acetamiprid was greatly enhanced by DNA in the range of pH 1.6-1.8. A RLS peak at 313 nm was found, and the enhanced intensity of RLS at this wavelength was proportional to the concentration of DNA. The linear range of the calibration curve was 0-11.0 microg ml(-1) with the detection limit of 20 ng ml(-1). The nucleic acids in synthetic sample and in rice seedling extraction were determined satisfactorily. The interaction mechanism of acetamiprid and DNA is discussed. Mechanism studies show that the enhanced RLS is due to the aggregation of acetamiprid in the presence of DNA.     

蛋白质-SDS-罗丹明B体系的共振光散射光谱及其分析应用

研究了阴离子表面活性剂十二烷基硫酸钠(SDS),阳离子染料罗丹明B,与蛋白质相互作用的共振光散射(RLS)光谱及用于蛋白质的测定.实验表明,在pH 4.35的酸性介质中,SDS的共振光散射强度较小,它与蛋白质结合后,共振光散射强度能得到增强,但加入阳离子染料罗丹明B后,共振光散射强度显著增强.在λ=332.0 nm处,ΔIRLS最大,并且增强的共振光散射信号与蛋白质的浓度成正比.据此建立了一种测定蛋白质的新方法,该方法灵敏度高,对HSA的检出限达到1.9 ng/mL,线性范围为0.01～5.0 μg/mL.用于人血清样品中蛋白质的测定,回收率为94.0%～105.5%.     

Study on the interaction of nucleic acids with silver nanoparticles—Al(III) by resonance light scattering technique and its analytical application

It is found that Al(III) can further enhance the intensity of resonance light scattering (RLS) of the silver nanoparticles (AgNPs) and nucleic acids system. Based on this, a novel method of determination of nucleic acids is proposed in this paper. Under optimum conditions, there are linear relationships between the enhancing extent of RLS and the concentration of nucleic acids in the range of 1.0 × 10⁻⁹-1.0 × 10⁻⁷ g mL⁻¹, 1.0 × 10⁻⁷-2.0 × 10⁻⁶ g mL⁻¹ for fish sperm DNA (fsDNA), 1.0 × 10⁻⁹-7.0 × 10⁻⁸ g mL⁻¹ for calf thymus DNA (ctDNA) and 1.0 × 10⁻⁹-1.0 × 10⁻⁷ g mL⁻¹ for yeast RNA (yRNA). The detection limits (S/N = 3) of fsDNA, ctDNA and yRNA are 4.1 × 10⁻¹⁰ g mL⁻¹, 4.0 × 10⁻¹⁰ g mL⁻¹ and 4.5 × 10⁻¹⁰ g mL⁻¹, respectively. The studies indicate that the RLS enhancement effect should be ascribed to the formation of AgNPs-Al(III)-DNA aggregations through electrostatic attraction and adsorption bridging action of Al(III). And the sensitivity and stability of the AgNPs-fsDNA system could be enhanced by Al(III).     

虎红-牛血清白蛋白共振光散射光谱研究及其分析应用

基于在pH3.0的BR缓冲溶液中蛋白质的加入使虎红的共振光散射信号增强,建立了一种蛋白质测定的新方法.详细地探讨了pH、染料用量、表面活性剂、离子强度、共存物质等对信号的影响.牛血清白蛋白浓度在0～4.0μg/mL范围内与体系散射强度呈线性关系,检出限为0.01718μg/mL.该方法用于合成样品中牛血清白蛋白的测定,...     

Study on the resonance Rayleigh scattering spectra and resonance non-linear spectra of congo red-amikacin system and its analytical application

The interaction between congo red (CR) and amikacin (AMK) was studied by resonance Rayleigh scattering (RRS), frequency doubling scattering (FDS) and second-order scattering (SOS) combining with absorption spectrum. In a weak acidic medium, CR combined with AMK to form an ion association complex with the composition ratio of 1∶1 by electrostatic interaction, hydrophobicity and charge transferring effect. As a result, the new spectra of RRS, FDS, and SOS appeared and their intensities were enhanced greatly. The maximum wavelengths of RRS, FDS and SOS were located at 563 nm, 475 nm and 940 nm, and the scattering intensities were proportional to the concentration of AMK. These three methods have very high sensitivities, and the detection limits were 4.0 ng·mL?1 for RRS, 3.6 ng·mL?1 for FDS and 1.9 ng·mL?1 for SOS, respectively. At the same time, the methods have better selectivity. A new method for the determination of trace amounts of AMK with congo red by resonance scattering technique has been developed. The recovery for the determination of AMK in blood serum and urine sample was between 95.5% and 105.5%. In this study, the properties, such as enthalpy of formation, charge distribution and mean polarizability, were calculated by AM1 quantum chemistry method. In addition, the reaction mechanism and the reasons for the enhancement of scattering spectra were discussed.     

A study on the interaction between concanavalin A and glycogen by light scattering technique and its analytical application

The mixture of concanavalin A (Con A) and glycogen shows strong light scattering character. Based on it, the interaction between Con A and glycogen was studied on a common spectrofluorimeter by light scattering technique. Many factors affecting the light scattering intensity (LSI), such as pH, temperature, reaction time, ion strength and the denaturing agent of protein were studied in detail. Experimental results showed that the LSI reached its maximum after mixing Con A with glycogen for about 20 min in pH 7.4 Tris-HCl buffer at 37 degrees C. The results also suggested that the conformation of Con A was critical for its unique binding affinity to glycogen. Electrostatic forces should not be the primary interaction between glycogen and Con A. Under proper experimental conditions, the determination method for glycogen by light scattering technique was developed. The glycogen determination can be performed in the range of 0.48-32.0, 0.50-32.0 and 0.32-24.0 mug/ml for Rabbit liver glycogen (RL Gly), Oyster glycogen (O Gly) and Clam Glycogen (C Gly), respectively. The influence of co-existing substances such as proteins, mono- and di-saccharides and metal ions was evaluated, and little interference came from the foreign substances. The determinations of glycogen in synthetic samples demonstrated that the recovery rate was in the range of 98.1-103% and the relative standard deviations (RSD) were lower than 5.0%.     

Ru（bpy）3^2＋ -DNA体系的共振光散射光谱研究及其分析应用

研究了Ru(bpy)32 与脱氧核糖核酸(DNA)作用的共振光散射光谱。基于DNA对Ru(bpy)32 共振光散射的增强效应,建立了共振光散射法测定DNA的新方法。在最佳实验条件下,Ru(bpy)32 在373nm处的共振光散射增强与DNA的质量浓度呈线性关系,线性范围为0.04~3.2μg/mL,检出限为16ng/mL。应用于合成样品及实际样品中DNA的测定。     

甲基紫与苋菜红相互作用的双波长共振光散射比率光谱研究及其分析应用

应用双波长共振光散射比率法(DW-RLS)研究了甲基紫与苋菜红之间的相互作用.在pH 1.24的乙酸钠-HCl缓冲溶液中,甲基紫和苋菜红本身的共振光散射(RLS)信号均很弱,但是当它们相互作用形成缔合物时,导致RLS信号明显增强并出现新的RLS光谱,适当浓度的Triton X-100存在使结合反应敏化,缔合物最大散射峰位于528 nm,RLS信号强度与苋菜红的浓度呈线性关系.通过测量528 nm处的RLS强度或两个波长处RLS强度比值(I417/I343),可对苋菜红进行定量检测.当溶液中甲基紫的浓度为1.54×10-5 mol/L时,RLS法测定苋菜红的线性范围和检出限分别为0.05～0.50 μg/mL和0.02 μg/mL,而DW-RLS法的线性范围和检出限分别为0.01～0.60 μg/mL和1 ng/mL,与RLS法相比较,DW-RLS法受酸度、离子强度等环境条件影响较小,并且有更宽的线性范围和更低的检出限.     

中性红-8-羟基喹啉-亚硝酸根体系共振散射光谱研究及分析应用

NO2-与中性红在HCl介质中发生重氮化反应,生成的重氮盐在弱碱性溶液中与8-羟基喹啉发生偶联反应,偶联产物使得位于588 nm的共振散射光强度明显增强.基于该重氮化-偶联反应建立了共振散射光谱法测定NO2-的新方法.激光散射法测得样品中偶联反应产物的平均粒径为493 nm.方法的线性范围和检出限分别为0～480×10-6 g/L和8.9×10-6 g/L.方法用于蔬菜中NO2-的测定,回收率在95.9%～102.1%.     

Determination of dextrin based on its self-aggregation by resonance light scattering technique

A novel free-probe assay of dextrin was established based on the resonance light scattering (RLS) enhancement in aqueous solution due to the self-aggregation of dextrin. The RLS intensity was well proportional to the concentration of dextrin over the wide range 0.2-14 μg mL⁻¹ and a detection limit 0.02 μg mL⁻¹ was obtained in the optimum conditions. The effect factors such as pH, buffer medium, holding time, ionic strength and temperature were studied in detail. Little or no interference was presented in the detection when adding coexisting substances including various metal ions and some saccharine in the solution. The assay proposed owns the advantages of easy operation, rapidity, sensitivity and practicability. Three synthetic samples and three kinds of medicine samples were analyzed with satisfactory results.     

Resonance light scattering of 1-hydroxypyrene-ethyl violet-anionic surfactant system and its analytical application.

A novel method for the rapid and sensitive analysis of 1-hydroxypyrene (1-OHP) in human urine has been developed that uses a resonance light scattering (RLS) technique. The assay was based on the interaction of ethyl violet (EV) with 1-hydroxypyrene to form an ion-associate complex, which resulted in the enhancement of RLS intensity and the appearance of new RLS spectra. In the presence of anionic surfactant, the maximum RLS peak of the system was located at 396 nm at pH 8.0. Under the optimum conditions, it was found that the enhanced RLS intensity was directly proportional to the concentration of 1-hydroxypyrene in the range of 4.0 - 982 microg l(-1). The detection limit was 1.2 microg l(-1) and the recoveries of 1-hydroxypyrene were 92.8 - 102.3% (n = 6). The proposed method was successfully applied to the analysis of human urine samples. The results of 1-hydroxypyrene were in agreement with those obtained by the method of high-performance liquid chromatography.     

溴化十六烷基三甲铵存在下固红VR盐与fsDNA作用的共振光散射增强研究及其分析应用

研究了在阳离子表面活性剂溴化十六烷基三甲铵(CTMAB)存在下, 阴离子染料固红VR盐(FVR)和鱼精脱氧核糖核酸(fsDNA)作用的共振光散射(RLS)光谱特性、影响因素和最佳反应条件. 在pH 5.72和离子强度低于0.01 mol/L的条件下, fsDNA和CTMAB对FVR的共振光散射光谱有协同增强作用, 产生最大散射波长为361 nm的共振光散射增强(RLSE)信号. 在优化实验条件下, 测定fsDNA的线性范围为0.01～2.0 mg/L, 检出限可达2.5 μg/L. 方法能用于合成样中DNA的测定.     

光散射分析技术测定盐酸环丙沙星含量

在pH 4.6的乙酸-乙酸钠缓冲溶液中,环丙沙星能与四苯硼钠作用生成沉淀产生光散射信号(LS)能应用普通荧光分光光度计检测,从而建立了环丙沙星的光散射分析法.LS光谱在385.0 nm处,具有特征散射峰,且增强的光散射强度(ΔILS)与0.03～0.2 μg/mL,0.2～2.5 μg/mL两个范围内的环丙沙星溶液呈线性关系,相对应的检出限分别为7.4,2.7 ng/mL.本实验中研究了酸度、聚乙二醇600溶液的浓度、四苯硼酸钠溶液的浓度以及共存物质对LS强度的影响.方法已用于盐酸环丙沙星片剂中环丙沙星的测定,RSD为0.3%～0.6%.     

Study on bromocresol green-cetyltrimethylammonium-deoxyribonucleic acids system by resonance light scattering spectrum methods

An assay of deoxyribonucleic acids (DNA) determination, with the sensitivity at nanogram level, was established in the present study by using a common spectrofluorometer to detect the intensity of resonance light scattering (RLS). In hexamethylene tetramine (HMTA) buffer (pH 11.00), Bromocresol Green (BCG) and deoxyribonucleic acids (DNA) react with cetyltrimethylammonium bromide (CTMAB) to form large particles of three-component complex, which results in strong enhanced RLS signals characterized by three peaks at 336, 390, and 622 nm and at 336 nm that is the strongest of the three enhanced RLS peaks. Mechanistic studies showed that the enhanced RLS stems from the aggregation of BCG on DNA through the bridged and synergistic effect of CTMAB. Yeast DNA (yDNA), in the range of 0.05-0.90 ngml(-1), fish sperm DNA (fsDNA) in the range of 0.05-0.80 ngml(-1), and calf thymus DNA (ctDNA) in the range of 0.05-0.80 ngml(-1) can be determined if 2.0 x 10(-6) moll(-1) BCG was employed. The determination limit of yDNA was 12.7 ngml(-1). Three synthetic samples of yDNA were analyzed with good reproducibility.     

共振光散射光谱法测定马来酸氯苯那敏

在pH 4.3的HAc-NaAc缓冲溶液中,荧光桃红与马来酸氯苯那敏依靠静电引力和疏水作用力形成离子缔合物,导致体系共振光散射增强.讨论了共振光散射增强的原因,并考察了一些因素对体系的影响.在最佳实验条件下,增强的共振光散射强度与马来酸氯苯那敏的浓度在0.2～12.0 μg/mL范围内呈良好线性关系,检出限为0.047...     

甲醇-水、乙醇-水体系聚集态的共振散射光谱

自从Ｐａｓｔｅｒｎａｃｋ[1,2]使用普通荧光分光光度计建立共振光散射(ＲＬＳ)技术以来,人们用该技术建立了十分灵敏的蛋白质和核酸的分析方法[3,5]。同时该技术在研究化合物在溶液中的聚集态方面也有了较为广泛的应用,一般认为分子聚集体的形成是引起ＲＬＳ增强的主要原因[6]。已知甲醇、乙醇与水互溶形成均匀的溶液体系,那么在这些溶液体系中是否也存在某种形式的分子聚集体呢?为此本文研究了不同浓度的甲醇水溶液和乙醇水溶液的ＲＬＳ光谱。1　实验部分1 1　试剂和仪器甲醇(上海建鑫化工试剂厂,分析纯,含量%≥99 5);乙醇(安徽特酒总…